Process for producing alloys containing zirconium



Patented Mar. 18, i941 I Q PROCESS FOR PRODUCING ALLOYS CONTAINING ZIRCONIUM Helmut von Zeppelin, Bitterfeld, and Ludwig Teichmann, Leverkusen-I. G. Wei-k, Germany, assignors, by mesne assignments, to Walther H. Duisberg, New York, N. Y.

No Drawing. Application January 18, 1940, Se-

rial No, 314,451. In Germany January 24,

. 4 Claims. (Cl. 75-g-177) This invention relates to the production of ally comprise a-sallne'residue of magnesium chicloys containing zirconium. ride and an alkali metal chloride; and finely di- The production of alloys containing zirconium vided zirconium metal distributed therein, are by standard methods, .e. g. by introducing zirdirectly contacted with the molten base metal 5 conium metal in pulverulent form, into a molten of the zirconium alloy to be formed. The reaccharge of the base metal is, because of the tendtion mixture may be employed with the saline ency of irconium t l powder t i nite, only residue either fused or solidified. When employfeasible when operating in an inert atmosphere ing the former alternative, then the fused saline or in vacuo, and even then only with considerable residue containing the zirconium metal in susprecaution. Moreover, commercial zirconium pension is simply poured on the molten base 10 metal frequently contains a certain percentage metal and carefully stirred thereinto. It is, of impurities such as hydrogen, oxygen, and however, always preferable first to allow the zirnitrogen (the latter two generally in the form conium metal produced by the reaction to settle of oxides or nitrides),.which impurities become from the fused saline residue and then to disincorporated in the zirconium metal in the course card the bulk of the latter so that only that por- 15 of its production on its being separated from retion of the mixture which contains the zirconium action residues, which is generally efiected by a metal in somewhatconcentrated form is used for treatment with acids. When employing zircoalloying purposes. The separation of the bulk nium metal containing the aforesaid impurities, of the saline residue from the portion containing 30 for alloying purposes, We have observed that the the settled zirconium metal may be effected either alloying proceeds very slowly, so that it is deby decantingthe fused saline residue off the said sirable to use a zirconium metal for alloying purpart, or by allowing the entire reaction mixture poses in which the aforesaid impurities are abto solidify after settling, whereupon the cake is sent. I divided into the aforesaid two portions, e. g. by

33 It is an object of our present invention to procutting. The cake can then be broken up and vide a process for the production of alloys constrewn on and carefully stirred into the molten taining zirconium which is not attended with the base metal. The saline residue introduced along aforesaid disadvantages, i. e. whichwill enable with the zirconium metal forms a covering on the alloying operation to proceed smoothly and the alloy which protects the latter from undemore rapidly and without undue oxidation of the sirable reaction with the constituents of the atzirconium metal. mosphere, and incidentally alsoserves as a flux;

In our copending application S. N. 314,450, the dissolution of the zirconium metal in the base entitled Production of zirconium metal, and filed metal is thus enabled to take place with the on even date herewith, we have disclosed and greatest rapidity.

, claimed a process for the production of zirco- The efiiciency of the reaction mixtures con- 5 nium metal, wherein a mixture comprising a taining zirconium metal and produced in acquantity of zirconium chloride, 9. quantity of an ccrdance with our copending application, for n alkali metal chloride by weight at least about loying purposes, is probably due to the fact that equal to half the charge of zirconium chloride, any reaction of the zirconium metal such as 10 and further a quantity of magnesium metal is oxydation is prevented by the particles of zirheated, so as to cause reduction of the zirconium ni metal being and remaining completely chloride by the magnesium, whereupon the saline surrounded by the saline residue until the zirmelt is separated from the zirconium metal proconium. is taken up by the base metal.

duced.

We have now ascertained that the mixtures Example obtained as a result of the reaction described in 1.5 kgs. of a reaction mixture produced in acour copending application, which mixtures comcordance with our copending application S. N. prise zirconium metal in pulverulent form and 314,450 and consisting of 33.4% by weight of a saline residue comprising magnesium chloride P s um Chloride, by weight of magneand an alkali metal chloride, are a very efficient slum chloride and 29.4% by Weight 0f conium 50 means for producing alloys containing zircoetal Particles. balance impurities, are intronium. I duced into 20 kgs. of a zinciferous magnesium According to our present invention reaction base alloy heated to 770 C., while stirring. The mixtures of the kind obtained in the process of stirring is cdntinued for about 1 minute there- .35 our copending application which thus essentialafter, whereupon the whole is allowed to settle.

The molten metal is then poured while keeping back the slag, and the alloy obtained then contains 0.5% of zirconium.

We claim:

1. A process for producing alloys containing zirconium, which comprises causing to contact with the molten metal to be alloyed with zirconium, a product consisting of finely divided particles of zirconium metal dispersed in a mixture of magnesium chloride and an alkali metal chloride.

2. A process for producing alloys containing zirconium, which comprises causing to contact with the molten metal to be alloyed with zirconium, a product consisting of finely divided particles of zirconium metal dispersed in a mix- .ture of magnesium chloride and an alkali metal chloride, said product having been produced by reaction of zirconium chloride with magnesium in the presence of said alkali metal chloride.

3. A process for producing alloys containing zirconium, which comprises introducing, while carefully stirring, into the molten metal to be alloyed with zirconium a product consisting of finely divided particles of zirconium metal dispersed in a mixture of magnesium chloride and an alkali metal chloride, said product having been produced by reaction of zirconium chloride with magnesium in the presence of said alkali metal chloride.

4. A process for producing a magnesium base alloy containing zinc and zirconium, which comprises introducing, while carefully stirring, into the liquid alloy of magnesium and zinc, a product consisting of finely divided particles of zirconium metal dispersed in a saline melt of magnesium chloride and an alkali metal chloride, said product having been produced by reaction of zirconium chloride with magnesium in the presence of said alkali metal chloride.

HELMUT VON ZEPPELIN. LUDWIG TEICHMANN. 

